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Ammonia → HCID 69330037, 화합물

HRID 1351835
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HRID 1351835 반응식
[OH:1][C:2]1[CH:38]=[CH:37][C:5]2[CH2:6][CH2:7][CH2:8][CH:9]([N:11]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:12][C@H:13]([O:22][Si:23]([CH2:28][CH3:29])([CH2:26][CH3:27])[CH2:24][CH3:25])[CH2:14][O:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:10][C:4]=2[CH:3]=1.[N:39]1[CH:44]=CC=CC=1.ClC(OC1C=CC([N+]([O-])=O)=CC=1)=[O:47].N>ClCCl.CN(C)C1C=CN=CC=1.C(O)C.O>[O:15]([CH2:14][C@@H:13]([O:22][Si:23]([CH2:26][CH3:27])([CH2:24][CH3:25])[CH2:28][CH3:29])[CH2:12][N:11]([C:30]([O:32][C:33]([CH3:35])([CH3:34])[CH3:36])=[O:31])[CH:9]1[CH2:8][CH2:7][CH2:6][C:5]2[CH:37]=[CH:38][C:2]([O:1][C:44](=[O:47])[NH2:39])=[CH:3][C:4]=2[CH2:10]1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 222AmmoniaHCID 1049PyridineHCID 821294-Nitrophenyl chloroformateHCID 57157362HCID 57157362, 화합물

생성물 1

HCID 69330037HCID 69330037, 화합물

시약·촉매·용매 4

HCID 142844-(Dimethylamino)pyridine촉매
HCID 702
Ethanol
용매
HCID 962Water용매
HCID 6344Dichloromethane용매

실험 절차

Under nitrogen, to a solution of N-(3-hydroxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)-N-[(2S)-3-phenoxy-2-(triethylsilyloxy)propyl]-tert-butoxycarbonylamine (150 mg) in dichloromethane (5 ml) were added pyridine (64 ml), 4-nitrophenyl chloroformate (116 mg) and a catalytic amount of 4-dimethylaminopyridine at 5° C. After being stirred at the same temperature for 2 hours, to this one was added about 6.8M ammonia in ethanol (0.5 ml), and the mixture was stirred at room temperature for 12 hours. The resulting mixture was pured into water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1) to give N-[(2S)-3-phenoxy-2-(triethyl-silyloxy)propyl]-N-[3-carbamoyloxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl]-tert-butoxycarbonylamine (129 mg).

후처리

  1. customat 5° C
  2. stirringthe mixture was stirred at room temperature for 12 hours
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-1731f07921f3474a821e2571159fd423
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07217706B2

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